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Preparation method of nitrogen-phosphorus double-doped hollow carbon nanotube

A carbon nanotube, double doping technology, applied in chemical instruments and methods, electrical components, circuits, etc., can solve the problems of ineffective utilization of the inner wall and uneven distribution of nitrogen elements in carbon nanotubes, and increase the reactive sites. , low cost, high electrocatalytic activity

Inactive Publication Date: 2017-10-20
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims to solve the shortcomings of current nitrogen-containing carbon nanotubes, such as nitrogen-doped carbon nanotubes, binary nitrogen-doped carbon nanotubes, etc., and the uneven distribution of nitrogen elements caused by the bamboo-like structure of nitrogen-containing carbon nanotubes. To solve the problem that the inner wall of carbon nanotubes cannot be effectively utilized, it provides a simple and feasible method for preparing hollow nitrogen-phosphorus double-doped carbon nanotubes with uniform distribution of nitrogen and phosphorus and effective use of the inner wall by using nickel phosphide catalysis

Method used

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  • Preparation method of nitrogen-phosphorus double-doped hollow carbon nanotube
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  • Preparation method of nitrogen-phosphorus double-doped hollow carbon nanotube

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Embodiment 1

[0027] A method for preparing nitrogen-phosphorus double-doped hollow carbon nanotubes, the operation is as follows:

[0028] (1) Soak the nickel foam in hydrogen peroxide with a mass concentration of 30%, while maintaining the temperature at 60°C for heat treatment for 10 hours, so that the surface of the nickel-based material is oxidized to generate nickel hydroxide, and then the amino trimethylene phosphonic acid resin is tiled Put it on a porcelain boat, and cover it with the nickel-based material obtained after heat treatment;

[0029] (2) Transfer the material boat obtained in step (1) into a tube furnace, keep the heating rate in a nitrogen atmosphere at 5°C / min and heat to 850°C for 0.5 hour heat treatment, the compound in the material boat is provided by thermal decomposition Gaseous carbon source, nitrogen source and phosphorus source, phosphating reaction occurs on the surface of the nickel-based material and nickel phosphide is generated, and the cylindrical nickel...

Embodiment 2

[0032] A method for preparing nitrogen-phosphorus double-doped hollow carbon nanotubes, the operation is as follows:

[0033] (1) Soak the nickel sheet in hydrogen peroxide with a mass concentration of 15%, while maintaining the temperature at 40°C for 6 hours, so that the surface of the nickel-based material is oxidized to form nickel hydroxide, and then spread the cyanamide phosphoric acid resin on the porcelain boat On, and cover the nickel-based material obtained after heat treatment;

[0034] (2) Transfer the material boat obtained in step (1) into a tube furnace, maintain a heating rate of 5°C / min in an inert atmosphere nitrogen and heat it to 700°C for heat treatment for 3.5 hours, and the compound in the material boat is thermally decomposed Provide gaseous carbon source, nitrogen source and phosphorus source, phosphating reaction occurs on the surface of the nickel-based material and nickel phosphide is generated, and the cylindrical nickel phosphide catalyzes the gro...

Embodiment 3

[0037] A method for preparing nitrogen-phosphorus double-doped hollow carbon nanotubes, the operation is as follows:

[0038] (1) Soak the nickel foil in hydrogen peroxide with a mass concentration of 23%, while maintaining the temperature at 80°C for heat treatment for 2 hours to oxidize the surface of the nickel-based material to generate nickel hydroxide, and then spread (triphenylphosphine) acetonitrile Put it on a porcelain boat, and cover it with the nickel-based material obtained after heat treatment;

[0039](2) Transfer the material boat obtained in step (1) into a tube furnace, keep the heating rate in an inert atmosphere argon at 5°C / min and heat to 1200°C for heat treatment for 2.0 hours, the compound in the material boat is heated Decompose to provide gaseous carbon source, nitrogen source and phosphorus source. Phosphating reaction occurs on the surface of nickel-based materials and nickel phosphide is generated. Cylindrical nickel phosphide catalyzes the growth ...

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Abstract

The invention discloses a preparation method of a nitrogen-phosphorus double-doped hollow carbon nanotube. The method comprises the following steps: soaking a nickel-based material in hydrogen peroxide in mass concentration of 15-30%, carrying out heating treatment for 2-10 hours at the temperature of 40-80 DEG C, and oxidizing the surface of the nickel-based material to generate nickel hydroxide. The method is capable of thermally decomposing the compound containing nitrogen and phosphorus; compared with the conventional nanotube containing nitrogen and carbon, the nitrogen-phosphorus double-doped hollow carbon nanotube prepared by the method has obvious structure advantages; the method is simple in reaction equipment, easily achievable and controllable in reaction conditions and low in cost; the prepared nitrogen-phosphorus double-doped hollow carbon nanotube has the structure advantage, shows high electrocatalytic activity extremely close to the commercial platinum carbon and more remarkable stability in oxygen reduction reaction of negative electrodes of fuel cells, and has great economic value and social value.

Description

technical field [0001] The invention relates to the field of carbon materials, in particular to a method for preparing a nitrogen-phosphorus double-doped hollow carbon nanotube. Background technique [0002] Oxidogen reaction is the core reaction process of future clean and efficient energy storage systems, and it is widely used in technologies such as fuel cells, metal-air batteries, and electrolyzed water. Due to its superior structure and unique physical and chemical properties, carbon nanotubes have shown potential application value in hydrogen storage, supercapacitors, fuel cell catalysts, etc., and have attracted extensive attention from researchers. Doping carbon nanotubes with heteroatoms such as nitrogen, boron, phosphorus, and sulfur can significantly improve the electrocatalytic activity of carbon nanotubes in the fuel cell cathode oxygen reduction reaction [J Phys Chem.2011, 115, 3769; Angewandte Chemie.2013, 125,3192]. In 2009, the team of Professor Dai Liming...

Claims

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Application Information

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IPC IPC(8): B01J27/24H01M4/90
CPCH01M4/9075B01J27/24B01J35/33Y02E60/50
Inventor 朱金良马少健沈培康
Owner GUANGXI UNIV
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